Synthesis and structure of tetraphenylphosphonium 2,4-dinitrobenzenesulfonate
Автор: Sharutin V.V., Mukusheva N., Urzhumova A.V.
Журнал: Вестник Южно-Уральского государственного университета. Серия: Химия @vestnik-susu-chemistry
Рубрика: Химия элементоорганических соединений
Статья в выпуске: 2 т.10, 2018 года.
Бесплатный доступ
The interaction of the solvate of pentaphenylphosphorus(Ph5P·½C6H6) with 2,4-dinitrobenzenesulfonic acid in a benzene solution synthesized tetraphenylphosphonium 2,4-dinitrobenzenesulfonate [Ph4P]+[O3SC6H3(NO2-2,4)]-(1), thermally stable (mp 185 °C), readily soluble in water, acetone, alcohol, dioxane, tetrahydrofuran, benzene, toluene, xylene and insoluble in aliphatic hydrocarbons. According to the X-ray diffraction data, obtained at 293 K for colorless crystals 1 [С30H23N2O7PS, M 586.53, the rhombic system, symmetry group P 212121, crystal size 0.15x0.20x0.25 mm, the data acquisition area 2θ, 6.02-34.98 degrees, intervals of reflection indexes -6 ≤h ≤ 6, -14 ≤ k ≤ 14, -18 ≤ l ≤ 18, total reflections 12782, independent reflections 1717, reflections with F2 > 2s(F2) 1663, Rint 0.0266, variables 370, GOOF 1.080, R1 = 0.0222, wR 2 = 0.0535, residual electron density 0.12 / -0.17 e / Å3] they consist of slightly distorted tetrahedral cations [the P-C bond lengths vary in the intervals 1.783(4)-1.801(4) Å; angles CPC are 106.31(19)°-110.54(19)°] and 2,4-dinitrobenzenesulfonate anions [distances S-O 1.443(3) -1.451(3) Å, S-С 1.813(4) Å; angles OSO 113.36(16)°-114.72(16)°, OSS 104.14(17)°]. Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data Bank (No. 1822547; deposit@ccdc.cam.ac.uk; http: //www.ccdc. Cam.ac.uk). The IR spectrum 1 contains absorption bands characteristic of sulfonic groups: 1227-1238 cm-1, 1141-1188 cm-1 and ~1000 cm-1. The action of potassium iodide aqueous solution on aqueous solution 1 leads to quantitative formation of tetraphenylphosphonium iodide.
[ph4p]+ [oso2с6h3(no2)2-2, complex, synthesis, x-ray diffraction analysis
Короткий адрес: https://sciup.org/147160426
IDR: 147160426 | DOI: 10.14529/chem180206